Search results for: solution combustion synthesis

Authors: Daniela Istrati, Alina Morosan, Maria Stanca, Bogdan Purcareanu, Adrian Fudulu, Laura Olariu, Alice Buteica, Ion Mindrila, Rodica Cristescu, Dan Eduard Mihaiescu

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Our present work is related to the synthesis, characterization and applications of new nanocomposite materials based on silica mesoporous nanocompozites systems. The nanocomposite support was obtained by using a specific step–by–step multilayer structure buildup synthetic route, characterized by XRD (X-Ray Difraction), TEM (Transmission Electron Microscopy), FT-IR (Fourier Transform-Infra Red Spectrometry), BET (Brunauer–Emmett–Teller method) and loaded with Salvia officinalis plant extract obtained by a hydro-alcoholic extraction route. The sustained release of the target compounds was studied by a modified LC method, proving low release profiles, as expected for the high specific surface area support. The obtained results were further correlated with the in vitro / in vivo behavior of the nanocomposite material and recommending the silica mesoporous nanocomposites as good candidates for biomedical applications. Acknowledgements: This study has been funded by the Research Project PN-III-P2-2.1-PTE-2016-0160, 49-PTE / 2016 (PROZECHIMED) and Project Number PN-III-P4-ID-PCE-2016-0884 / 2017.

Keywords: biomedical, mesoporous, nanocomposites, natural products, sustained release

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Authors: Deniz Bozoglu, Deniz Deger, Kemal Ulutas, Sahin Yakut

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In recent years, silica aerogels have attracted great attention due to their outstanding properties, and their wide variety of potential applications such as microelectronics, nuclear and high-energy physics, optics and acoustics, superconductivity, space-physics. Hydrophobic silica aerogels were successfully synthesized in one-step by surface modification at ambient pressure. FT-IR result confirmed that Si-OH groups were successfully converted into hydrophobic and non-polar Si-CH3 groups by surface modification using trimethylchloro silane (TMCS) as co-precursor. Using Alpha-A High-Resolution Dielectric, Conductivity and Impedance Analyzer, AC conductivity of samples were examined at temperature range 293-423 K and measured over frequency range between 1-106 Hz. The characteristic relaxation time decreases with increasing temperature. The AC conductivity follows σ_AC (ω)=σ_t-σ_DC=Aω^s relation at frequencies higher than 10 Hz, and the dominant conduction mechanism is found to obey the Correlated Barrier Hopping (CBH) mechanism. At frequencies lower than 10 Hz, the electrical conduction is found to be in accordance with DC conduction mechanism. The activation energies obtained from AC conductivity results and it was observed two relaxation regions.

Keywords: aerogel, synthesis, dielectric constant, dielectric loss, relaxation time

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Authors: E. M. AbdelRazek, G. S. ElBahy, M. A. Allam, A. M. Abdelghany, A. M. Hezma

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Polymeric biocomposite of hydroxyapatite/polyacrylic acid were prepared and their thermal and mechanical properties were improved by addition of cellulose acetate. FTIR spectroscopy technique and X-ray diffraction analysis were employed to examine the physical and chemical characteristics of the biocomposites. Scanning electron microscopy shows a uniform distribution of HAp nano-particles through the polymeric matrix of two organic/inorganic composites weight ratios (60/40 and 70/30), at which the material crystallinity reaches a considerable value appropriate for the needed applications were studied and revealed that the HAp nano-particles are uniformly distributed in the polymeric matrix. Kinetic parameters were determined from the weight loss data using non isothermal thermogravimetric analysis (TGA). Also, the main degradation steps were described and discussed. The mechanical properties of composites were evaluated by measuring tensile strength and elastic modulus. The data indicate that the addition of cellulose acetate can make homogeneous composites scaffold significantly resistant to higher stress. Elastic modulus of the composites was also improved by the addition of cellulose acetate, making them more appropriate for bioapplications.

Keywords: biocomposite, chemical synthesis, infrared spectroscopy, mechanical properties

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Authors: Raja Asad Zaheer, Aisha Tanveer, Hafza Mehreen Fatima

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Global Software Development (GSD) is becoming a common norm in software industry, despite of the fact that global distribution of the teams presents special issues for effective communication and coordination of the teams. Now trends are changing and project management for distributed teams is no longer in a limbo. GSD can be effectively established using agile and project managers can use different agile techniques/tools for solving the problems associated with distributed teams. Agile methodologies like scrum and XP have been successfully used with distributed teams. We have employed exploratory research method to analyze different recent studies related to challenges of GSD and their proposed solutions. In our study, we had deep insight in six commonly faced challenges: communication and coordination, temporal differences, cultural differences, knowledge sharing/group awareness, speed and communication tools. We have established that each of these challenges cannot be neglected for distributed teams of any kind. They are interlinked and as an aggregated whole can cause the failure of projects. In this paper we have focused on creating a scalable framework for detecting and overcoming these commonly faced challenges. In the proposed solution, our objective is to suggest agile techniques/tools relevant to a particular problem faced by the organizations related to the management of distributed teams. We focused mainly on scrum and XP techniques/tools because they are widely accepted and used in the industry. Our solution identifies the problem and suggests an appropriate technique/tool to help solve the problem based on globally shared knowledgebase. We can establish a cause and effect relationship using a fishbone diagram based on the inputs provided for issues commonly faced by organizations. Based on the identified cause, suitable tool is suggested, our framework suggests a suitable tool. Hence, a scalable, extensible, self-learning, intelligent framework proposed will help implement and assess GSD to achieve maximum out of it. Globally shared knowledgebase will help new organizations to easily adapt best practices set forth by the practicing organizations.

Keywords: agile project management, agile tools/techniques, distributed teams, global software development

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Authors: R. M. W. Rajapakshe

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Sri Lanka, which is officially called the Democratic Socialist Republic of Sri Lanka is an island nation situated near India. It is a multi-lingual, multi- religious and multi – ethnic country, where Sinhalese form the majority and the Tamils form the largest ethnic minority. The composition of the population (ethnic basis) in Sri Lanka is as follows: Sinhalese: 74.5%, Tamil (Sri Lankan): 12.6%, Muslim: 7.5 %, Tamil (Indian): 5.5%, Malay: 0.3%, Burgher: 0.3 %, other: 0.2 %. The Tamil people use the Tamil language as their mother tongue and the Sinhala people use the Sinhala language as their mother tongue. A very few people in both communities use English as their mother tongue and however, a large number of people use English as a second language. The Sinhala Language was declared the only official language in Sri Lanka in 1959. However, it was not acceptable to Tamil politicians as well as to the common Tamil people and it was the beginning of long standing ethnic crisis which later became a military war where a lot of blood was shed. As a solution to the above ethnic crisis the thirteenth amendment to the constitution of Sri Lanka was introduced in 1987 and according to it both Sinhala and Tamil were declared official languages and English as the link language in Sri Lanka. Thus, a new programme namely, second language teaching programme under which Sinhala was taught to Tamil students and Tamil was taught to Sinhala students, was introduced at government schools. Language teaching includes knowledge of the culture of the target language. As all cultures are mixed and have common features students have reduced their enmity about the other community and learned to respect the other culture. On the other hand as all languages are mixed, students came to the understanding that there are no pure languages. Thus, they learned to respect the other language. In the case of Sri Lanka the Sinhala language is mixed with the Tamil language and vice versa. Thus, the development of second language teaching is the prominent way to solve the above ethnic problem and this study clearly shows it. However, the above programme suffers with lack of trained second language teachers, infrastructure facilities and insufficient funds and, they can be considered as the main obstacles to develop the second language teaching programme. Yet, there are no satisfactory answers to those problems. The data were collected from relevant books, articles and other documents based on research and forty five recordings, each with one hour duration, of natural conversations covering all factions of the Sinhala community.

Keywords: ethnic crisis, official language, second language teaching, Sinhala, Tami

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Authors: C. Benhamideche

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Fluoroaluminate glasses have been reported as the earliest heavy metal fluoride glasses. By comparison with flurozirconate glasses, they offer a set of similar optical features, but also some differences in their elastic and chemical properties. In practice they have been less developed because their stability against devitrification is smaller than that of the most stable fluoroziconates. The purpose of this study was to investigate glass formation in systems AlF3-YF3-PbF2-MgF2-MF2 (M= Li, Na, K). Synthesis was implemented at room atmosphere using the ammonium fluoride processing. After fining, the liquid was into a preheated brass mold, then annealed below the glass transition temperature for several hours. The samples were polished for optical measurements. Glass formation has been investigated in a systematic way, using pseudo ternary systems in order to allow parameters to vary at the same time. We have chosen the most stable glass compositions for the determination of the physical properties. These properties including characteristic temperatures, density and proprieties elastic. Glass stability increases in multicomponent glasses. Bulk samples have been prepared for physical characterization. These glasses have a potential interest for passive optical fibers because they are less sensitive to water attack than ZBLAN glass, mechanically stronger. It is expected they could have a larger damage threshold for laser power transmission.

Keywords: fluoride glass, aluminium fluoride, thermal properties, density, proprieties elastic

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Authors: Madhurima Poddar, Vinay Sharma, Shaikh M. Mobin, Rajneesh Misra

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Three 1,8-naphthalimide (NPI) substituted 4,4-difluoroboradiaza-s-indacene (BODIPY) dyads were synthesized via Pd-catalyzed Sonogashira cross-coupling reaction of ethynyl substituted NPI with the meso-, β- and α-halogenated BODIPYs, respectively. The photophysical and electrochemical data reveals considerable electronic communication between the BODIPY and NPI moieties. The electronic absorption spectrum reveals that the substitution of NPI at α position of BODIPY exhibit better electronic communication between the NPI and the BODIPY units. The electronic structures of all the dyads exhibit planar geometries which are in a good correlation with the structures obtained from single crystal X-ray diffraction. The crystal structures of the dyads exhibit interesting supramolecular interactions. The dyads show good cytocompatibility with the potential of multicolor live-cell imaging; making them excellent candidates for biological applications. The work provides an important strategy of screening the substitution pattern at different position of BODIPYs which will be useful for the design of BODIPY based organic molecules for various optoelectronic applications as well as bio-imaging.

Keywords: bio-imaging studies, cross-coupling, cyclic voltammetry, density functional calculations, fluorescence spectra, single crystal XRD, UV/Vis spectroscopy

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Authors: Chhavi Saxena

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FinFETs can be a replacement for bulk-CMOS transistors in many different designs. Its low leakage/standby power property makes FinFETs a desirable option for memory sub-systems. Memory modules are widely used in most digital and computer systems. Leakage power is very important in memory cells since most memory applications access only one or very few memory rows at a given time. As technology scales down, the importance of leakage current and power analysis for memory design is increasing. In this paper, we discover an option for low power interconnect synthesis at the 32nm node and beyond, using Fin-type Field-Effect Transistors (FinFETs) which are a promising substitute for bulk CMOS at the considered gate lengths. We consider a mechanism for improving FinFETs efficiency, called variable supply voltage schemes. In this paper, we’ve illustrated the design and implementation of FinFET based 4x4 SRAM cell array by means of one bit 7T SRAM. FinFET based 7T SRAM has been designed and analysis have been carried out for leakage current, dynamic power and delay. For the validation of our design approach, the output of FinFET SRAM array have been compared with standard CMOS SRAM and significant improvements are obtained in proposed model.

Keywords: FinFET, 7T SRAM cell, leakage current, delay

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Authors: P. Shrivastava, S. Vijayalakshmi, A. K. Singh, S. Dalai, R. Teotia, P. Sharma, J. Bellare

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This paper focuses on the synthesis and application of nanobioactive glass for bone regeneration studies. Nanobioactive glass has been synthesized by sol gel method having a combination of silicon, calcium and phosphorous in the molar ratio of 75:21:4. The prepared particles were analyzed for surface morphology by FEG SEM and FEG TEM. Physiochemical properties were investigated using ICP AES, FTIR spectroscopy and X-ray diffraction (XRD) techniques. To ascertain their use for therapeutic use, biocompatibility evaluation of the particles was done by performing soaking studies in SBF and in vitro cell culture studies on MG63 cell lines. Cell morphology was observed by FE SEM and phase contrast microscopy. Nanobioactive glasses (NBG) thus prepared were of 30-200 nm in size, which makes them suitable for nano-biomedical applications. The spherical shape of the particles imparts high surface to volume ratio, promoting fast growth of hydroxyapatite (HA), which is the mineral component of bone. As evaluated by in vitro cell culture studies the NBG was found to enhance the surface activation which enhances osteoblast adhesion. This is an essential parameter to improve bone tissue integration, thereby making nanobioactive glass therapeutically suitable for correcting bone defects.

Keywords: biocompatibility, bone tissue engineering, hydroxyapatite, nanobioactive glass

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Authors: Demet Tatar, Bahattin Düzgün

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In this study, we have newly developed titanium-tin oxide (TiSnO) thin films as the transparent conducting oxides materials by the spray pyrolysis technique. Tin oxide thin films doped with different Ti content were successfully grown by spray pyrolysis and they were characterized as a function of Ti content. The effect of Ti contents on the crystalline structure and optical properties of the as-deposited SnO2:Ti films was systematically investigated by X-ray diffraction (XRD), scanning electronic microscopy (SEM), atomic force microscopy (AFM), UV-vis spectrometer and photoluminecenc spectrophotometer. The X-ray diffraction patterns taken at room temperature showed that the films are polycrystalline. The preferred directions of crystal growth appeared in the difractogram of SnO2: Ti (TiTO) films were correspond to the reflections from the (110), (200), (211) and (301) planes. The grain size varies from 21.8 to 27.8 nm for (110) preferred plane. SEM and AFM study reveals the surface of TiTO to be made of nanocrystalline particles. The highest visible transmittance (570 nm) of the deposited films is 80 % for 20 wt % titanium doped tin oxide films. The obtained results revealed that the structures and optical properties of the films were greatly affected by doping levels. These films are useful as conducting layers in electro chromic and photovoltaic devices.

Keywords: transparent conducting oxide, gas sensors, SnO2, Ti, optoelectronic, spray pyrolysis

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Authors: Zarana Dave

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Cerium-doped lanthanum bromide, LaBr₃ (Ce), scintillator shows attracting properties for spectroscopy that makes it a suitable solution for security, medical, geophysics and high energy physics applications. Here, the performance parameters of a cylindrical LaBr₃ (Ce) scintillator was investigated. The first aspect is the determination of the efficiency for γ - ray detection, measured with GEANT4 simulation toolkit from 10keV to 10MeV energy range. The second is the detailed study of background radiation of LaBr₃ (Ce). It has relatively high intrinsic radiation background due to naturally occurring ¹³⁸La and ²²⁷Ac radioisotopes.

Keywords: LaBr₃(Ce), GEANT4, efficiency, background radiation

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Authors: Rashid Mahmood, Muhammad Junaid Sarwar

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Mobile ad hoc networks (MANETs) use has been well-known from the last few years in the many applications, like mission critical applications. In the (MANETS) prevention method is not adequate as the security concerned, so the detection method should be added to the security issues in (MANETs). The authentication and encryption is considered the first solution of the MANETs problem where as now these are not sufficient as MANET use is increasing. In this paper we are going to present the concept of intrusion detection and then survey some of major intrusion detection techniques in MANET and aim to comparing in some important fields.

Keywords: MANET, IDS, intrusions, signature, detection, prevention

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Authors: G. G. Kagramanov, E. N. Farnosova, Linn Maung Maung

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The technologies of ion exchange and nanofiltration can be used for treatment of wastewater containing copper and other heavy metal ions to decrease the environmental risks. Nanofiltration characteristics under water treatment of heavy metals have been studied. The influence of main technical process parameters - pressure, temperature, concentration and pH value of the initial solution on flux and rejection of nanofiltration membranes has been considered. And ion exchange capacities of resins in removal of heavy metal ions from wastewater have been determined.

Keywords: exchange capacity, heavy metals, ion exchange, membrane separation, nanofiltration

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Authors: Anuar Ishak

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The characteristics of fluid flow and heat transfer over a permeable shrinking sheet is studied. The governing partial differential equations are transformed into a set of ordinary differential equations, which are then solved numerically using MATLAB routine boundary value problem solver bvp4c. Numerical results show that dual solutions are possible for a certain range of the suction parameter. A stability analysis is performed to determine which solution is linearly stable and physically realizable.

Keywords: dual solutions, heat transfer, shrinking sheet, stability analysis

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Authors: Lawrence Mzukisi Madikizela, Luke Chimuka

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Removal of organics from wastewater offers a better water quality, therefore, the purpose of this work was to investigate the use of molecularly imprinted polymer (MIP) for the elimination of selected organics from water. A multi-template MIP for the adsorption of naproxen, ibuprofen and diclofenac was synthesized using a bulk polymerization method. A MIP was synthesized at 70°C by employing 2-vinylpyridine, ethylene glycol dimethacrylate, toluene and 1,1’-azobis-(cyclohexanecarbonitrile) as functional monomer, cross-linker, porogen and initiator, respectively. Thermogravimetric characterization indicated that the polymer backbone collapses at 250°C and scanning electron microscopy revealed the porous and roughness nature of the MIP after elution of templates. The performance of the MIP in aqueous solutions was evaluated by optimizing several adsorption parameters. The optimized adsorption conditions were 50 mg of MIP, extraction time of 10 min, a sample pH of 4.6 and the initial concentration of 30 mg/L. The imprinting factors obtained for naproxen, ibuprofen and diclofenac were 1.25, 1.42, and 2.01, respectively. The order of selectivity for the MIP was; diclofenac > ibuprofen > naproxen. MIP showed great swelling in water with an initial swelling rate of 2.62 g/(g min). The synthesized MIP proved to be able to adsorb naproxen, ibuprofen and diclofenac from contaminated deionized water, wastewater influent and effluent.

Keywords: adsorption, molecularly imprinted polymer, multi template, pharmaceuticals

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Authors: Maja Andrić, Josip Pečarić

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Over the last five decades, an enormous amount of work has been done on Opial’s integral inequality, dealing with new proofs, various generalizations, extensions and discrete analogs. The Opial inequality is recognized as a fundamental result in the analysis of qualitative properties of solution of differential equations. We use submultiplicative convex functions, appropriate representations of functions and inequalities involving means to obtain generalizations and extensions of certain known multidimensional integral and discrete Opial-type inequalities.

Keywords: Opial's inequality, Jensen's inequality, integral inequality, discrete inequality

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Authors: Alemu Tadesse Feroche

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In this study, some 2, 3 distributed quinazoline -4 (3H) - one derivative were synthesized using a three-step synthetic route. They were obtained in a good yield (59.5-85%) by applying different chemical reactions like cyclization and condensation reactions. The chemical structure of the final compounds was also verified by spectroscopic methods (IR, ¹HNMR) and elemental microanalysis. The in vivo antimalarial activity of these compounds on P. berghei infected mice was found to be moderate to high at an oral dose of 0.04846 mmol/kg /day. This is equal to 25 mg/kg of chloroquine phosphate, which causes 100% inhibition of the parasite. It is worth mentioning that most active compounds (E) -3 Phenyl -2- [2- (pyridine -4- yl) vinyl] -4 (3H) -quinazolinone IVa (64.02%, (E)-2-[2-(4 - Hydroxy-3 - methoxystyryl) - vinyl) -3 - phenyl -4 (3H ) - quinazolinone IVc (77.25%) and (E)-2 –[2 –(Pyridin -4-yl) –vinyl] -3 phenenylamine -4(3H) quinazolinone IVe (73.54%) showed a dose-dependent increase in present suppression in antimalarial activities. Furthermore, the synthesized compounds were screened for their in vitro antileishmanial activity against L. aethiopica isolate (CL/039/09). All tested compounds (IVa (0.03766 ug/ml), IVb (0.00538 ug/ml, IVc (0.00412 ug/ml, IVd (0.00110 ug/ml), IVe (0.03017 ug/ml) and IVf (0.03894 ug/ml)) showed excellent potency that is much better than amphotericin B (IC50 = 0,04359 ug/ml). The results of acute toxicity indicated that all test compounds (IVa –IVf) proved to be nontoxic and well tolerated by the experimental animals up to 300 mg/kg in oral and 140 mg/kg in parental studies.

Keywords: 4(3H)-quinazolinone, in vivo antimalarial activity, in vitro antileishmanial activity, acute toxicity

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Authors: Abderrahim Siam, Ramdane Maamri, Zaidi Sahnoun

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The development of adaptive user interfaces (UI) presents for a long time an important research area in which researcher attempt to call upon the full resources and skills of several disciplines. The adaptive UI community holds a thorough knowledge regarding the adaptation of UIs with users and with contexts of use. Several solutions, models, formalisms, techniques, and mechanisms were proposed to develop adaptive UI. In this paper, we propose an approach based on the fuzzy set theory for modeling the concept of the appropriateness of different solutions of UI adaptation with different situations for which interactive systems have to adapt their UIs.

Keywords: adaptive user interfaces, adaptation solution’s appropriateness, fuzzy sets

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Authors: Ashiq Hussain, Mahwash Hussain, Zeenat Parveen

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Now a days the demand for broadband service has increased. Due to which the researchers are trying to find a solution to provide a large amount of service. There is a shortage of bandwidth because of the use of downloading video, voice and data. One of the solutions to overcome this shortage of bandwidth is to provide the communication system with passive optical components. We have increased the data rate in this system. From experimental results we have concluded that the quality factor has increased by adding passive optical networks.

Keywords: WDM-PON, optical fiber, BER, Q-factor, eye diagram

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Authors: Aziza Altaibayeva, Ertan Güdekli, Ratbay Myrzakulov

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In this letter, we explore exact solutions for the Horava-Lifshitz gravity. We use of an extension of this theory with first order dynamical lapse function. The equations of motion have been derived in a fully consistent scenario. We assume that there are some spherically symmetric families of exact solutions of this extended theory of gravity. We obtain exact solutions and investigate the singularity structures of these solutions. Specially, an exact solution with the regular horizon is found.

Keywords: quantum gravity, Horava-Lifshitz gravity, black hole, spherically symmetric space times

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Authors: Yomna Ibrahim El-Gazzar, Hussien Ibrahim El-Subbagh, Hanan Hanaa Georgey, Ghada S. Hassan Hassan

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Dihydrofolate reductase (DHFR) is an enzyme that has pivotal importance in biochemistry and medicinal chemistry. It catalyzes the reduction of dihydrofolate to tetrahydrofolate and intimately couples with thymidylate synthase. Thymidylate synthase is a crucial enzyme that catalyzes the reductive methylation of (dUMP) to (dTMP) utilizing N5, N10-methylenetetrahydrofolate as a cofactor. A new series of 2-substituted thio-quinazolin-4-one analogs was designed that possessed electron withdrawing or donating functional groups (Cl or OCH3) at position 6- or 7-, 4-methoxyphenyl function at position 3-.The thiol function is used to connect to either 1,2,4-triazole, or 1,3,4-thiadiazole via a methylene bridge. Most of the functional groups designed to be accommodated on the quinazoline ring such as thioether, alkyl to increase lipid solubility of polar compounds, a character very much needed in the nonclassical DHFR inhibitors. The target compounds were verified with spectral data and elemental analysis. DHFR inhibitions, as well as antitumor activity, were applied on three cell lines (MCF-7, CACO-2, HEPG-2).

Keywords: nonclassical antifolates, DHFR Inhibitors, antitumor activity, quinazoline ring

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Authors: Claudia Aguilar, Amen Farooq

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Among other cities in the United States, the city of Atlanta is experiencing levels of growth that surpass anything we have witnessed in the last century. With the surge of population influx, the available housing is practically bursting at the seams. Supply is low, and demand is high. In effect, the average one-bedroom apartment runs for 1,800 dollars per month. The city is desperately seeking new opportunities to provide affordable housing at an expeditious rate. This has been made evident by the recent updates to the city’s zoning. With the recent influx in the housing market, young professionals, in particular millennials, are desperately looking for alternatives to stay within the city. To remedy Atlanta’s affordable housing crisis, the city of Atlanta is planning to introduce 40 thousand of new affordable housing units by 2026. To achieve the urgent need for more affordable housing, the architectural response needs to adapt to overcome this goal. A method that has proven successful in modern housing is to practice modular means of development. A method that has been constrained to the dimensions of the max load for an eighteen-wheeler. This approach has diluted the architect’s ability to produce site-specific, informed design and rather contributes to the “cookie cutter” stigma that the method has been labeled with. This thesis explores the design methodology for modular housing by revisiting its constructability and adaptability. This research focuses on a modular housing type that could break away from the constraints of transport and deliver adaptive reconfigurable assemblies. The adaptive assemblies represent an integrated design strategy for assembling the future of affordable dwelling units. The goal is to take advantage of a component-based system and explore a scalable solution to modular housing. This proposal aims specifically to design a kit of parts that are made to be easily transported and assembled but also gives the ability to customize the use of components to benefit all unique conditions. The benefits of this concept could include decreased construction time, cost, on-site labor, and disruption while providing quality housing with affordable and flexible options.

Keywords: adaptive assemblies, modular architecture, adaptability, constructibility, kit of parts

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Authors: Silvana Caglieri

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Theoretical study of acetylation of p-methylaniline catalyzed by Cu2+ ions from the analysis of intermediate of the reaction was carried out. The study of acetylation of amines is of great interest by the utility of its products of reaction and is one of the most frequently used transformations in organic synthesis as it provides an efficient and inexpensive means for protecting amino groups in a multistep synthetic process. Acetylation of amine is a nucleophilic substitution reaction. This reaction can be catalyzed by Lewis acid, metallic ion. In reaction mechanism, the metallic ion formed a complex with the oxygen of the acetic anhydride carbonyl, facilitating the polarization of the same and the successive addition of amine at the position to form a tetrahedral intermediate, determining step of the rate of the reaction. Experimental work agreed that this reaction takes place with the formation of a tetrahedral intermediate. In the present theoretical work were investigated the structure and energy of the tetrahedral intermediate of the reaction catalyzed by Cu2+ ions. Geometries of all species involved in the acetylation were made and identified. All of the geometry optimizations were performed by the method at the DFT/B3LYP level of theory and the method MP2. Were adopted the 6-31+G* basis sets. Energies were calculated using the Mechanics-UFF method. Following the same procedure it was identified the geometric parameters and energy of reaction intermediate. The calculations show 61.35 kcal/mol of energy for the tetrahedral intermediate and the energy of activation for the reaction was 15.55 kcal/mol.

Keywords: amides, amines, DFT, MP2

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Authors: Anthony P. Anies, Jose C. Muñoz

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A new shortcut method for the design of reactive-dividing wall columns (RDWC) is proposed in this work. The RDWC is decomposed into its thermodynamically equivalent configuration naming the Petlyuk column, which consists of a reactive prefractionator and an unreactive main fractionator. The modified FUGK(Fenske-Underwood-Gilliland-Kirkbride) shortcut distillation method, which incorporates the effect of reaction on the Underwood equations and the Gilliland correlation, is used to design the reactive prefractionator. On the other hand, the conventional FUGK shortcut method is used to design the unreactive main fractionator. The shortcut method is applied to the synthesis of dimethyl ether (DME) through the liquid phase dehydration of methanol, and the results were used as the starting design inputs for rigorous simulation in Aspen Plus V8.8. A mole purity of 99 DME in the distillate stream, 99% methanol in the side draw stream, and 99% water in the bottoms stream were obtained in the simulation, thereby making the proposed shortcut method applicable for the preliminary design of RDWC.

Keywords: aspen plus, dimethyl ether, petlyuk column, reactive-dividing wall column, shortcut method, FUGK

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Authors: Eko S. Kunarti, Akhmad Syoufian, Indriana Kartini, Agnes

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Fe₃O₄/SiO₂/TiO₂ nanoparticles have been synthesized and applied as a photocatalyst for the recovery of gold from the mixture of Au(III) and Cu(II) ions. The synthesis was started by the preparation of magnetite (Fe₃O₄) using coprecipitation and sonication methods, followed by SiO₂ coating on magnetite using sol-gel reactions, and then TiO₂ coating using sol-gel process. Characterization was performed by using infrared spectroscopy, X-ray diffraction, transmission electron microscopy methods. Activity of Fe₃O₄/SiO₂/TiO₂ nanoparticles was evaluated as a photocatalyst for recovery of gold through photoreduction of Au(III) ions in Au(III) and Cu(II) ions mixture with a ratio of 1:1, in a closed reactor equipped with UV lamp. The photoreduction yield was represented as a percentage (%) of reduced Au(III) which was calculated by substraction of initial Au(III) concentration by the unreduced one. The unreduced Au(III) was determined by atomic absorption spectrometry. Results showed that the Fe₃O₄/SiO₂/TiO₂ nanoparticles were successfully synthesised with excellent magnetic and photocatalytic properties. The nanoparticles present optimum activity at a pH of 5 under UV irradiation for 120 minutes. At the optimum condition, the Fe₃O₄/SiO₂/TiO₂ nanoparticles could reduce Au³⁺ to Au⁰ 97.24%. In the mixture of Au(III) and Cu(II) ions, the Au(III) ions are more easily reducible than Cu(II) ions with the reduction results of 96.9% and 45.80% for Au(III) and Cu(II) ions, respectively. In addition, the presence of Cu(II) ions has no significant effect on the amount of gold recovered and its reduction reaction rate.

Keywords: Fe₃O₄/SiO₂/TiO₂, photocatalyst, recovery, gold, Au(III) and Cu(II) mixture

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Authors: Littlelet N. Scarlet, Kamaluddin Abdur-Rashid, Paul T. Maragh, Tara Dasgupta

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Aminophosphines are a privileged class of ancillary ligands with emerging importance in homogeneous catalysis. The unique combination of soft phosphorus (P) and hard nitrogen (N) centres affords a variety of transition metal complexes as potential pre-catalysts for synthetically useful reactions. Herein three ligand systems will be reported; two bidentate ligands - (S)-8-(diphenyl-phosphino)-1,2,3,4-tetrahydronaphthalen-1-amine, (S)THNANH2, and (Rc)-1-((Sp)-2-diphenylphosphino) ferrocenylethylamine, (RcSp)PPFNH2 - and a tridentate (Rc)-1-((Sp)-2-diphenylphosphino) ferrocenylimino-pyridine, (RcSp)PPFNNH2 ligand; the latter prepared from the condensation of selected ferrocene aminophosphines with pyridine-2-carboxaldehyde. Suitable combinations of these aminophosphine ligands with ruthenium precursors have afforded highly efficient systems for the asymmetric hydrogenation and transfer hydrogenation of selected ketones in 2-propanol. The Ru-(S)THNANH2 precatalyst was the most efficient in the asymmetric hydrogenation of selected ketones with 100% conversions within 4 hours at a catalyst loading of 0.1 mol%. The Ru-(RcSp)PPFNNH2 precatalyst was the most efficient in the asymmetric transfer hydrogenation of the ketones with conversions as high as 98% with 0.1 mol% catalyst. However, the enantioselectivities were generally low.

Keywords: aminophosphine, asymmetric hydrogenation, homogeneous catalysis, ruthenium (II), transfer hydrogenation

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Authors: Agman Gupta, Rajashekar Badam, Noriyoshi Matsumi

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Introduction: Recently, silicon has been recognized as one of the potential alternatives as anode active material in Li-ion batteries (LIBs) to replace the conventionally used graphite anodes. Silicon is abundantly present in the nature, it can alloy with lithium metal, and has a higher theoretical capacity (~4200 mAhg-1) that is approximately 10 times higher than graphite. However, because of a large volume expansion (~400%) upon repeated de-/alloying, the pulverization of Si particles causes the exfoliation of electrode laminate leading to the loss of electrical contact and adversely affecting the formation of solid-electrolyte interface (SEI).1 Functional polymers as binders have emerged as a competitive strategy to mitigate these drawbacks and failure mechanism of silicon anodes.1 A variety of aqueous/non-aqueous polymer binders like sodium carboxy-methyl cellulose (CMC-Na), styrene butadiene rubber (SBR), poly(acrylic acid), and other variants like mussel inspired binders have been investigated to overcome these drawbacks.1 However, there are only a few reports that mention the attempt of addressing all the drawbacks associated with silicon anodes effectively using a single novel functional polymer system as a binder. In this regard, here, we report a novel highly robust n-type bisiminoacenaphthenequinone (BIAN)-paraphenylene-based crosslinked polymer as a binder for Si anodes in lithium-ion batteries (Fig. 1). On its application, crosslinked-BIAN binder was evaluated to provide mechanical robustness to the large volume expansion of Si particles, maintain electrical conductivity within the electrode laminate, and facilitate in the formation of a thin SEI by restricting the extent of electrolyte decomposition on the surface of anode. The fabricated anodic half-cells were evaluated electrochemically for their rate capability, cyclability, and discharge capacity. Experimental: The polymerized BIAN (P-BIAN) copolymer was synthesized as per the procedure reported by our group.2 The synthesis of crosslinked P-BIAN: a solution of P-BIAN copolymer (1.497 g, 10 mmol) in N-methylpyrrolidone (NMP) (150 ml) was set-up to stir under reflux in nitrogen atmosphere. To this, 1,6-dibromohexane (5 mmol, 0.77 ml) was added dropwise. The resultant reaction mixture was stirred and refluxed at 150 °C for 24 hours followed by refrigeration for 3 hours at 5 °C. The product was obtained by evaporating the NMP solvent under reduced pressure and drying under vacuum at 120 °C for 12 hours. The obtained product was a black colored sticky compound. It was characterized by 1H-NMR, XPS, and FT-IR techniques. Results and Discussion: The N 1s XPS spectrum of the crosslinked BIAN polymer showed two characteristic peaks corresponding to the sp2 hybridized nitrogen (-C=N-) at 399.6 eV of the diimine backbone in the BP and quaternary nitrogen at 400.7 eV corresponding to the crosslinking of BP via dibromohexane. The DFT evaluation of the crosslinked BIAN binder showed that it has a low lying lowest unoccupied molecular orbital (LUMO) that enables it to get doped in the reducing environment and influence the formation of a thin (SEI). Therefore, due to the mechanically robust crosslinked matrices as well as its influence on the formation of a thin SEI, the crosslinked BIAN binder stabilized the Si anode-based half-cell for over 1000 cycles with a reversible capacity of ~2500 mAhg-1 and ~99% capacity retention as shown in Fig. 2. The dynamic electrochemical impedance spectroscopy (DEIS) characterization of crosslinked BIAN-based anodic half-cell confirmed that the SEI formed was thin in comparison with the conventional binder-based anodes. Acknowledgement: We are thankful to the financial support provided by JST-Mirai Program, Grant Number: JP18077239

Keywords: self-healing binder, n-type binder, thin solid-electrolyte interphase (SEI), high-capacity silicon anodes, low-LUMO

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Authors: Dionisios Panagiotaras, Dimitrios Papoulis, Elias Stathatos

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Microfibrous palygorskite and tubular halloysite clay mineral combined with nanocrystalline TiO2 are incorporating in the preparation of nanocomposite films on glass substrates via sol-gel route at 450 °C. The synthesis is employing nonionic surfactant molecule as pore directing agent along with acetic acid-based sol-gel route without addition of water molecules. Drying and thermal treatment of composite films ensure elimination of organic material lead to the formation of TiO2 nanoparticles homogeneously distributed on the palygorskite or halloysite surfaces. Nanocomposite films without cracks of active anatase crystal phase on palygorskite and halloysite surfaces are characterized by microscopy techniques, UV-Vis spectroscopy, and porosimetry methods in order to examine their structural properties. The composite palygorskite-TiO2 and halloysite-TiO2 films with variable quantities of palygorskite and halloysite were tested as photocatalysts in the photo-oxidation of Basic Blue 41 azo dye in water. These nanocomposite films proved to be most promising photocatalysts and highly effective to dye’s decoloration in spite of small amount of palygorskite -TiO2 or halloysite- TiO2 catalyst immobilized onto glass substrates mainly due to the high surface area and uniform distribution of TiO2 on clay minerals avoiding aggregation.

Keywords: halloysite, palygorskite, photocatalysis, titanium dioxide

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Authors: Tânia F. C. V. Silva, Eloísa S. S. Vieira, João Pinto da Costa, Rui A. R. Boaventura, Vitor J. P. Vilar

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Sanitary landfill leachates are characterized as a complex mixture of diverse organic and inorganic contaminants, which are usually removed by combining different treatment processes. Due to its simplicity, reliability, high cost-effectiveness and high nitrogen content (mostly under the ammonium form) inherent in this type of effluent, the activated sludge biological process is almost always applied in leachate treatment plants (LTPs). The purpose of this work is to assess the effect of the main nitrification and denitrification variables on the nitrogen's biological removal, from mature leachates. The leachate samples were collected after an aerated lagoon, at a LTP nearby Porto, presenting a high amount of dissolved organic carbon (1.0-1.3 g DOC/L) and ammonium nitrogen (1.1-1.7 g NH4+-N/L). The experiments were carried out in a 1-L lab-scale batch reactor, equipped with a pH, temperature and dissolved oxygen (DO) control system, in order to determine the reaction kinetic constants at unchanging conditions. The nitrification reaction rate was evaluated while varying the (i) operating temperature (15, 20, 25 and 30ºC), (ii) DO concentration interval (0.5-1.0, 1.0-2.0 and 2.0-4.0 mg/L) and (iii) solution pH (not controlled, 7.5-8.5 and 6.5-7.5). At the beginning of most assays, it was verified that the ammonium stripping occurred simultaneously to the nitrification, reaching up to 37% removal of total dissolved nitrogen. The denitrification kinetic constants and the methanol consumptions were calculated for different values of (i) volatile suspended solids (VSS) content (25, 50 and 100 mL of centrifuged sludge in 1 L solution), (ii) pH interval (6.5-7.0, 7.5-8.0 and 8.5-9.0) and (iii) temperature (15, 20, 25 and 30ºC), using effluent previously nitrified. The maximum nitrification rate obtained was 38±2 mg NH4+-N/h/g VSS (25ºC, 0.5-1.0 mg O2/L, pH not controlled), consuming 4.4±0.3 mg CaCO3/mg NH4+-N. The highest denitrification rate achieved was 19±1 mg (NO2--N+NO3--N)/h/g VSS (30ºC, 50 mL of sludge and pH between 7.5 and 8.0), with a C/N consumption ratio of 1.1±0.1 mg CH3OH/mg (NO2--N+NO3--N) and an overall alkalinity production of 3.7±0.3 mg CaCO3/mg (NO2--N+NO3--N). The denitrification process showed to be sensitive to all studied parameters, while the nitrification reaction did not suffered significant change when DO content was changed.

Keywords: mature sanitary landfill leachate, nitrogen removal, nitrification and denitrification parameters, lab-scale activated sludge biological reactor

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Authors: Asabe Ahmad Tijani, Y. A. Yahaya

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The paper considers the derivation of implicit Adams-Moulton type method, with k=4 and 5. We adopted the method of interpolation and collocation of power series approximation to generate the continuous formula which was evaluated at off-grid and some grid points within the step length to generate the proposed block schemes, the schemes were investigated and found to be consistent and zero stable. Finally, the methods were tested with numerical experiments to ascertain their level of accuracy.

Keywords: Adam-Moulton Type (AMT), off-grid, block method, consistent and zero stable

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